Beverages comprising stable granules of milled lutein

ABSTRACT

Beverages are provided which include a beverage liquid and granules mixed with the beverage liquid The granules include:(i) a milled carotenoid consisting of lutein and/or zeaxanthin, wherein the milled carotenoid has the following particle size distribution:D [3,2] in the range of from 0.6 to 1.5 μm, andD [v, 0.5] in the range of from 1.1 to 3.5 μm,(ii) a matrix material which encapsulates the milled carotenoid and comprises at least one modified food starch, a glucose syrup and sucrose, and(iii) a water-soluble antioxidant, whereinthe granules have the following particle size distribution:D [3,2] in the range of from 200 to 300 μm, andD [v, 0.5] in the range of from 220 to 320 μm, and whereinall D values are as measured by laser diffraction according to the Fraunhofer scattering model, and whereinthe granules do not include an oil or a gelatin.

CROSS-REFERENCE

This application is a divisional of commonly owned copending U.S. Ser.No. 16/086,458, filed Sep. 19, 2018 (now abandoned), which is the U.S.national phase of International Application No. PCT/EP2017/057814 filedApr. 3, 2017, which designated the U.S. and claims priority to CH PatentApplication No. 429/16 filed Apr. 1, 2016, the entire contents of eachof which are hereby incorporated by reference.

SUMMARY OF THE INVENTION

The present invention is directed towards the use of granules inbeverages, whereby the granules comprise

(i) a milled carotenoid selected from the group consisting of lutein andzeaxanthin and any mixture thereof having the following particle sizedistribution:

-   -   D [3,2] in the range of from 0.6 to 1.5 μm, and D [v, 0.5] in        the range of from 1.1 to 3.5 μm, and        (ii) a matrix comprising at least one modified food starch, a        glucose syrup and sucrose,        (iii) a water-soluble antioxidant,        wherein the granules have the following particle size        distribution:        D [3,2] in the range of from 200 to 300 μm, and D [v, 0.5] in        the range of from 220 to 320 μm,        all D values as measured by laser diffraction according to the        Fraunhofer scattering model,        whereby the milled carotenoid is encapsulated by the matrix.

The present invention is further directed towards the granules as suchand the beverages as such, as well as to a process for the manufactureof such granules.

Preferably the particle size distribution is measured after there-dispersed granules were treated with ultrasound and centrifuged.

The carotenoid is selected from the group consisting of lutein andzeaxanthin and any mixture thereof. Surprisingly the beveragescomprising granules of milled lutein according to the present inventionshow an intense yellow color.

Preferably the carotenoid is lutein. Lutein plays an important role ineye health. Thus, there is an increasing demand not only for dietarysupplements, especially in form of tablets, comprising lutein, but alsofor beverages being supplemented with lutein.

The water-soluble antioxidant is preferably sodium ascorbate.

Preferably the milled carotenoid has the following particle sizedistribution: D [3,2] is in the range of from 0.8 to 1.2 μm, preferablyD [3,2] is in the range of from 0.8 to 1.1 μm, as measured by laserdiffraction (Malvern Instruments Ltd, Malvern, UK, Mastersizer 3000)according to the Fraunhofer scattering model.

D [v, 0.5] is preferably in the range of from 1.1 to 2.6 μm, morepreferably D [v, 0.5] is in the range of from 1.1 to 2.1 μm, as measuredby laser diffraction (Malvern Instruments Ltd, Malvern, UK, Mastersizer3000) according to the Fraunhofer scattering model.

The particle size distribution of the granules is preferably as follows:

D [3,2] in the range of from 200 to 300 μm (preferably in the range offrom 230 to 270 μm) and D [v, 0.5] in the range of from 220 to 320 μm(preferably in the range of from 240 to 290 μm), all D values asmeasured by laser diffraction (Malvern Instruments Ltd, Malvern, UK,Mastersizer 3000) according to the Fraunhofer scattering model.

DETAILED DESCRIPTION OF THE INVENTION

Beverages According to the Present Invention

According to the present invention the granules of the milled carotenoid(especially lutein) with the preferences as given above can bepreferably used to color and/or fortify and/or supplement the followingbeverages: soft drinks as well as flavored waters, fortified waters,sports drinks, mineral drinks and carbonated beverages. Fruit juices andfruit-juice containing soft drinks may also be colored. Alcoholicbeverages, instant beverage powders, sugar-containing beverages and dietbeverages containing non-calorific or artificial sweeteners representstill further examples of beverages which can be colored and/orfortified and/or supplemented by the granules of the present invention.Such colored and/or fortified and/or supplemented beverages are alsoencompassed by the present invention, whereby flavored waters, softdrinks and sport drinks are preferred.

The soft drinks may be pasteurized or non-pasteurized. Usually they havea pH in the range of from 2 to 5, preferably in the range of from 2.5 to4, even more preferably in the range of from 2.8 to 3.6, i.e. that theyare acid.

The beverages according to the present invention comprise granules,whereby the granules comprise

(i) a milled carotenoid selected from the group consisting of lutein andzeaxanthin and any mixture thereof having the following particle sizedistribution:

-   -   D [3,2] in the range of from 0.6 to 1.5 μm, and D [v, 0.5] in        the range of from 1.1 to 3.5 μm, and        (ii) a matrix comprising at least one modified food starch, a        glucose syrup and sucrose,        (iii) a water-soluble antioxidant,        wherein the granules have the following particle size        distribution:        D [3,2] in the range of from 200 to 300 μm, and D [v, 0.5] in        the range of from 220 to 320 μm,        all D values as measured by laser diffraction according to the        Fraunhofer scattering model.

Amount of Milled Carotenoid in the Beverage

Preferably the amount of milled carotenoid (with the preferences asgiven above) in the beverage is in the range of from 1 ppm to 20 ppm,more preferably it is in the range of from 1 ppm to 15 ppm, mostpreferably it is in the range of from 1 ppm to 10 ppm, based on thetotal weight of the beverage.

The milled carotenoid is added to the beverage in the form of granulesaccording to the present invention.

The granules according to the present invention are now described inmore detail.

Granules According to the Present Invention

The present invention is directed towards granules comprising

(i) a milled carotenoid selected from the group consisting of lutein andzeaxanthin and any mixture thereof having the following particle sizedistribution:

-   -   D [3,2] in the range of from 0.6 to 1.5 μm, and D [v, 0.5] in        the range of from 1.1 to 3.5 μm, and        (ii) a matrix comprising at least one modified food starch, a        glucose syrup and sucrose,        (iii) a water-soluble antioxidant,        wherein the granules have the following particle size        distribution:

D [3,2] in the range of from 200 to 300 μm, and D [v, 0.5] in the rangeof from 220 to 320 μm,

all D values as measured by laser diffraction according to theFraunhofer scattering model.

The preferences for the particle size distribution have already beengiven above.

Carotenoid

The carotenoid is selected from the group consisting of lutein andzeaxanthin and any mixture thereof, more preferably the carotenoid islutein.

Lutein

As starting material most preferably a so-called “lutein cake” asavailable from Kemin Foods (US) having a lutein content of 50-80weight-% is used. This lutein cake is obtained by extracting MarigoldFlowers. The lutein cake also contains zeaxanthin, whereby the molarratio of the lutein to zeaxanthin is around 9:1. Lutein obtained fromany other natural source or by fermentation or by chemical synthesis mayalso be used.

Lutein extracted from natural sources often contains also certainamounts of zeaxanthin.

In a preferred embodiment of the present invention no other carotenoidexcept lutein and/or zeaxanthin is present. Excluded of this exceptionare carotenoids that may already be present in traces in the startingmaterial, e.g. in the “lutein cake”.

Amount of Carotenoid

The amount of the carotenoid is preferably in the range of from 1-30weight-%, more preferably in the range of from 5-25 weight-%, even morepreferably in the range of from 5-17 weight-%, most preferably in therange of from 10-17 weight-%, based on the total weight of the granules.

If the carotenoid is a mixture of lutein and zeaxanthin, their molarratio is preferably in the range of from 20:1 to 2:1, more preferablytheir molar ratio is in the range of from 10:1 to 4:1.

“Modified Food Starch”

A modified food starch is a food starch that has been chemicallymodified by known methods to have a chemical structure which provides itwith a hydrophilic and a lipophilic portion. Preferably the modifiedfood starch has a long hydrocarbon chain as part of its structure(preferably C5-C18).

One modified food starch is preferably used to make the granules of thisinvention, but it is also possible to use a mixture of two or moredifferent modified food starches.

Starches are hydrophilic and therefore do not have emulsifyingcapacities. However, modified food starches are made from starchessubstituted by known chemical methods with hydrophobic moieties. Forexample starch may be treated with cyclic dicarboxylic acid anhydridessuch as succinic anhydrides, substituted with a hydrocarbon chain (seeO. B. Wurzburg (editor), “Modified Starches: Properties and Uses, CRCPress, Inc. Boca Raton, Fla., 1986, and subsequent editions). Aparticularly preferred modified food starch of this invention has thefollowing formula (I)

wherein St is a starch, R is an alkylene radical and R′ is a hydrophobicgroup. Preferably R is a lower alkylene radical such as dimethylene ortrimethylene. R′ may be an alkyl or alkenyl group, preferably having 5to 18 carbon atoms. A preferred compound of formula (I) is an“OSA-starch” (starch sodium octenyl succinate). The degree ofsubstitution, i.e. the number of esterified hydroxyl groups to thenumber of free non-esterified hydroxyl groups usually varies in a rangeof from 0.1% to 10%, preferably in a range of from 0.5% to 4%, morepreferably in a range of from 3% to 4%.

The term “OSA-starch” denotes any starch (from any natural source suchas corn, waxy maize, waxy corn, wheat, tapioca and potato orsynthesized) that was treated with octenyl succinic anhydride (OSA). Thedegree of substitution, i.e. the number of hydroxyl groups esterifiedwith OSA to the number of free non-esterified hydroxyl groups usuallyvaries in a range of from 0.1% to 10%, preferably in a range of from0.5% to 4%, more preferably in a range of from 3% to 4%. OSA-starchesare also known under the expression “modified food starch”.

The term “OSA-starches” encompasses also such starches that arecommercially available e.g. from National Starch/Ingredion under thetradenames HiCap 100, Capsul (octenylbutanedioate amylodextrin), CapsulHS, Purity Gum 2000, Clear Gum Co03, UNI-PURE, HYLON VII; from NationalStarch/Ingredion and Roquette Freres, respectively; fromCereStar/Cargill under the tradename C*EmCap or from Tate & Lyle.

Amount of the Modified Food Starch/OSA Starch

The amount of the modified food starch (preferably the OSA starch) ispreferably in the range of from 10 to 50 weight-%, more preferably inthe range of from 25 to 45 weight-%, based on the total weight of thegranules.

Glucose Syrup

The glucose syrup can be used as such or in a dried form. Both arecommercially available starch hydrolysates, i.e. a mixture of mono-,oligo- and polysaccharides. According to the present invention a driedglucose syrup is preferably used. The preferences given for the driedglucose syrup apply also for the non-dried glucose syrup.

The term “dextrose equivalent” (DE) denotes the degree of hydrolysis andis a measure of the amount of reducing sugar calculated as D-glucosebased on dry weight; the scale is based on native starch having a DEclose to 0 and glucose having a DE of 100.

Dried glucose syrup is, as well as non-dried glucose syrup, usuallyclassified by its DE value, which is above 20. According to the presentinvention preferably a dried glucose syrup is used with a DE in therange of from 20 to 95, more preferably in the range of from 20 to 30,most preferably in the range of from 20 to 23.

In another embodiment of the present invention a mixture of two glucosesyrups is used—one having a low DE, preferably a DE 25, more preferablya DE in the range of from 20 to 25, and the other having a high DE,preferably a DE 90, more preferably a DE in the range of from 90 to 100.

Amount of Dried Glucose Syrup

The amount of the dried glucose syrup is in the range of from 0.1 to 40weight-%, preferably in the range of from 5 to 40 weight-%, morepreferably in the range of from 10 to 30 weight-%, most preferably inthe range of from 15 to 25 weight-%, based on the total weight of theformulation.

If non-dried glucose syrup is used, it is used in the same amount.

Sucrose (=Saccharose)

In a preferred embodiment of the present invention the weight ratio ofthe modified food starch to the dried glucose syrup to the sucrose is(1.5-2.5) to (0.5-1.5) to (0.5-1.5), more preferably it is (1.8-2.2) to(0.8-1.2) to (0.8-1.2), most preferably it is 2 to 1 to 1.

Amount of Sucrose

The amount of sucrose is preferably in the range of from 5 to 40weight-%, more preferably it is in the range of from 10 to 30 weight-%,most preferably it is in the range of from 15 to 25 weight-%, based onthe total weight of the granules.

In a preferred embodiment of the present invention the amount of thedried glucose syrup and the amount of sucrose is the same in kilograms.In a further preferred embodiment of the present invention the amount ofmodified food starch in kilograms is the same amount as the total amountof the dried glucose syrup and sucrose in kilograms.

Water-Soluble Anti-Oxidant

Preferably the water-soluble anti-oxidant is sodium ascorbate, but otherwater-soluble anti-oxidants being food-grade and thus, suitable forhuman consumption may also be used.

Amount of Water-Soluble Anti-Oxidant

The amount of waters-soluble anti-oxidant (especially sodium ascorbate)is preferably in the range of from 0.1 to 10 weight-%, more preferablyin the range of from 2 to 7 weight-%, most preferably in the range offrom 4 to 6 weight-%, based on the total weight of the granules.

The granules of the present invention may also contain up to 7 weight-%of water, preferably they contain up to 5 weight-% of water, based onthe total weight of the granules.

In a preferred embodiment of the present invention the amount of themilled carotenoid, the amount of the at least one modified food starch,the amount of the glucose syrup, the amount of sucrose and the amount ofthe water-soluble antioxidant (being preferably sodium ascorbate) sumpreferably up to an amount of at least 90 weight-%, preferably of atleast 95 weight-%, based on the total weight of the granules.

In an even more preferred embodiment of the present invention thegranules consist of the milled carotenoid, the at least one modifiedfood starch, the glucose syrup, sucrose, the water-soluble antioxidant(being preferably sodium ascorbate) and water.

In a further preferred embodiment of the present invention a lutein cakehaving a lutein content of 50-80 weight-% is used, whereby the weightratio of the lutein cake to the matrix consisting of the amount ofmodified food starch+dried glucose syrup+sucrose is 1: (4-6), preferably1: (4.8-5.5), more preferably 1 to (5-5.3).

In another preferred embodiment of the present invention a lutein cakehaving a lutein content of 50-80 weight-% is used, whereby the weightratio of the lutein cake to the modified food starch is 1 to (1.5-4),preferably 1 to (2-3), more preferably 1 to (2.5-2.7).

In a further preferred embodiment of the present invention a lutein cakehaving a lutein content of 50-80 weight-% is used, whereby the weightratio of the lutein cake to the dried glucose syrup is 1 to (0.5-2),preferably 1 to (1.0-1.5), more preferably 1 to (1.25-1.35).

In a further preferred embodiment of the present invention a lutein cakehaving a lutein content of 50-80 weight-% is used, whereby the weightratio of the lutein cake to sucrose is 1 to (0.5-2), preferably 1 to(1.0-1.5), more preferably 1 to (1.25-1.35).

Preferably no other compounds are present. Preferably no furtherhydrocolloids beside modified food starch and no further emulsifiers arepresent.

Compounds preferably not-being-present are the following ones:

-   -   Hydrolyzed lecithin products, especially those as disclosed on        page 5, line 5-19 of WO 2009/071295;    -   Gum Acacia; Gum Arabic as e.g. disclosed in WO 2007/009601; also        modified as disclosed in WO 2008/110225;    -   Gum Ghatti as e.g. described in WO 2009/147158;    -   Proteins such as gelatin (fish, swine, bovine gelatin);    -   Cellulose derivatives such as e.g. carboxmethylcellulose;    -   Plant proteins;    -   Milk proteins;    -   Ligninsulfonate;    -   Conjugates of plant gums and modified food starch, especially        those as disclosed in WO 2011/039336;    -   Sodium lauryl sulfate and other sodium alkyl sulfates;    -   Fat-soluble antioxidants such as e.g. dl-α-tocopherol;    -   Isomalt as e.g. used in the process of US 2008/0026124;    -   α-zeacarotene;    -   β-zeacarotene.

In an especially preferred embodiment of the present invention none ofthe following compounds is present in the granules:

-   -   Hydrolyzed lecithin products, especially those as disclosed on        page 5, line 5-19 of WO 2009/071295;    -   Gum Arabic as e.g. disclosed in WO 2007/009601;    -   Fat-soluble antioxidants such as e.g. dl-α-tocopherol;    -   Isomalt as e.g. used in the process of US 2008/0026124;    -   α-zeacarotene;    -   β-zeacarotene.

In a preferred embodiment the granules of the present invention do notcontain an oil. The term “oil” does not encompass any lipophilics thatmay be present in the granules, because they are part of the lutein cakeused as source of lutein.

The term “oil” in the context of the present invention encompassesglycerol and any triglyceride such as vegetable oils or fats like cornoil, sunflower oil, soybean oil, safflower oil, rapeseed oil, peanutoil, palm oil, palm kernel oil, cotton seed oil, olive oil or coconutoil or MCT (middle chain triglycerides) as well as any mixture thereof.

The oils can be from any origin. They can be natural, modified orsynthetic. The term “oil” in the context of the present invention thusalso encompasses canola oil, sesame oil, hazelnut oil, almond oil,cashew oil, macadamia oil, mongongo nut oil, pracaxi oil, pecan oil,pine nut oil, pistachio oil, sacha Inchi (Plukenetia volubilis) oil orwalnut oil.

The present invention also encompasses any combination of any preferredfeature of the milled carotenoid as mentioned in this patent applicationwith any preferred feature of the modified food starch, glucose syrup,sucrose, water-soluble antioxidant and also their preferred weightratios and the optional other ingredients of the granules as mentionedin this patent application though not explicitly mentioned.

Thus any combination of preferred embodiments of the present inventionis encompassed by the present invention though not explicitly mentioned.

The preferred granules of the present invention are granules comprisinga milled carotenoid in an amount in the range of from 1 to 30 weight-%(preferably 5 to 25 weight-%), at least one modified food starch in anamount in the range of from 10 to 50 weight-% (preferably 25 to 45weight-%), a glucose syrup in an amount in the range of from 0.1 to 40weight-% (preferably 10 to 30 weight-%), sucrose in an amount in therange of from 0.1 to 40 weight-% (preferably 10 to 30 weight-%), atleast one water-soluble antioxidant (preferably sodium ascorbate) in anamount in the range of from 0.1 to 10 weight-% (preferably 2 to 7weight-%) and water in an amount of from 0 to 7 weight-%, all amountsbeing based on the total amount of the granules, wherein the carotenoidis selected from the group consisting of lutein and zeaxanthin and anymixture thereof, and wherein the milled carotenoid has the followingparticle size distribution:

D [3,2] in the range of from 0.6 to 1.5 μm, and D [v, 0.5] in the rangeof from 1.1 to 3.5 μm, andwherein the granules have the following particle size distribution:D [3,2] in the range of from 200 to 300 μm, and D [v, 0.5] in the rangeof from 220 to 320 μm,all D values as measured by laser diffraction according to theFraunhofer scattering model,whereby the milled carotenoid is encapsulated by the matrix.

Further preferences of the compounds of the formulation of the presentinvention (milled carotenoid, modified food starch, glucose syrup,sucrose, water-soluble antioxidant and water) have already been givenabove.

Processes for the Manufacture of the Granules According to the PresentInvention

The granules according to the present invention are obtained accordingto the following process:

-   -   a) providing an aqueous solution of at least one modified food        starch, a glucose syrup and sucrose;    -   b) adding the carotenoid selected from the group consisting of        lutein and zeaxanthin and any mixture thereof to the solution of        step a) hereby obtaining a suspension;    -   c) milling the suspension of step b) until the following        particle size distribution of the milled carotenoid is reached:        -   D [3,2] in the range of from 0.6 to 1.5 μm and D [v, 0.5] in            the range of from 1.1 to 3.5 μm, both D values as measured            by laser diffraction (Malvern Instruments Ltd, Malvern, UK,            Mastersizer 3000) according to the Fraunhofer scattering            model;    -   d) spray-granulating the suspension of step c) to obtain        granules according to the present invention;        -   whereby a water-soluble antioxidant (preferably sodium            ascorbate) is added during the process.

Optionally a pH adjustment to a pH in the range of from 2.5 to 4.0(preferably in the range of from 2.9 to 3.5) may be carried out afterstep c). In a preferred embodiment of the present invention this pHadjustment step is carried out.

By this process granules are obtained which have preferably thefollowing particle size distribution:

D [3,2] in the range of from 200 to 300 μm (preferably in the range offrom 230 to 270 μm), D [v, 0.5] in the range of from 220 to 320 μm(preferably in the range of from 240 to 290 μm), both D values asmeasured by laser diffraction (Malvern Instruments Ltd, Malvern, UK,Mastersizer 3000) according to the Fraunhofer scattering model.

In a preferred embodiment of the present invention step d) is carriedout by drying the suspension obtained in step c) by fluid-bedgranulation.

Advantages of the Granules and Beverages of the Present Invention

The granules of the present invention have an excellent flowability sothey can be easily added to beverages.

The granules of the present invention show especially a flowability ofat least 100 g/min through an orifice with a diameter of 5 mm, and/or aflowability of at least 250 g/min through an orifice with a diameter of7 mm and/or a flowability of at least 500 g/min through an orifice witha diameter of 9 mm and/or a flowability of at least 700 g/min through anorifice with a diameter of 10 mm and/or a flowability of at least 2000g/min through an orifice with a diameter of 15 mm.

In a preferred embodiment the granules of the present invention show aflowability in the range of from 100 g/min to 150 g/min through anorifice with a diameter of 5 mm, and/or a flowability in the range offrom 250 g/min to 350 g/min through an orifice with a diameter of 7 mmand/or a flowability in the range of from 500 g/min to 750 g/min throughan orifice with a diameter of 9 mm and/or a flowability in the range offrom 700 g/min to 850 g/min through an orifice with a diameter of 10 mmand/or a flowability in the range of from 2000 g/min to 3000 g/minthrough an orifice with a diameter of 15 mm.

Advantageously the beverages containing the granules according to thepresent invention are color stable. Such beverages are especially softdrinks having a pH in the range of from 2 to 5, whereby the soft drinksmay be pasteurized or non-pasteurized.

“Color-stable” in the context of the present invention means that thecolor difference DE* between the initial color and the color after astorage time of 3 months should be lower than 10 (DE*<10). A DE*<10means that the color difference is in the acceptable area and underDE*<3 cannot be seen by naked eyes, i.e. without the use of an apparatussuch as a colorimeter.

The beverages, especially the soft drinks, containing the granulesaccording to the present invention show a color difference DE*1 over 60days.

Beverages, especially pasteurized and non-pasteurized soft drinks,according to the present invention comprising the granules according tothe present invention show a turbidity ≤150 NTU, preferably a turbidityin the range of from 100 to 150 NTU. The turbidity remains in this rangeeven after a storage time of up to 60 days. Furthermore, such softdrinks show a good chemical stability, meaning that the content oflutein is not decreasing below 80% of the initial value within a storagetime of 60 days.

The beverages, especially the pasteurized and non-pasteurized softdrinks, according to the present invention show also a very goodperformance with respect to their appearance attributes. That means that(almost) no ringing and (almost) no precipitation/sedimentation of thecarotenoid in the beverage occurs.

Such pasteurized and non-pasteurized soft drinks with 10 ppm of luteinshow a colour value L* in the range of from 85 to 95, a value a* in therange of from 3.0 to 5.5 and a value b* in the range of from 25 to 40.Preferably such pasteurized and non-pasteurized soft drinks with 10 ppmof lutein show a colour value L* in the range of from 88 to 91, a valuea* in the range of from 3.5 to 5.2 and a value b* in the range of from29 to 37. More preferably such pasteurized and non-pasteurized softdrinks with 10 ppm of lutein show a colour value L* in the range of from88.6 to 90.3, a value a* in the range of from 3.7 to 5.0 and a value b*in the range of from 29.4 to 36.6.

The invention is now further illustrated in the following non-limitingexamples.

EXAMPLES

The following abbreviations are used: RH=room humidity.

Example 1: Manufacture of Granules of Lutein and Zeaxanthin According tothe Present Invention

150 kg of OSA-Starch, 75 kg of dried glucose syrup and 75 kg of sucroseare dissolved in 440 l of preheated water at 72° C. for at least 30minutes (matrix). 60 kg of FloraGlo lutein crystals (as available fromKemin Foods, Des Moines, US) are then added to the matrix under stirringat a temperature between 36° C. and 20° C. After pH adjustment of theresulting suspension to a pH of 3.5 the resulting pH-adjusted suspensionis added to the milling beads (diameter of 0.3 mm) and milling iscarried out in several passages. To the resulting suspension 18 kg ofsodium ascorbate are added. Then water is added and spray drygranulation started. 275 kg of the granules are obtained.

Example 2: Manufacture of Granules of Lutein and Zeaxanthin According tothe Present Invention

160 kg of OSA-Starch, 80 kg of dried glucose syrup and 80 kg of sucroseare dissolved in 480 l of preheated water at 72° C. for at least 30minutes (matrix). 60 kg of FloraGlo lutein crystals (as available fromKemin Foods, Des Moines, US) are then added to the matrix under stirringat a temperature between 36° C. and 29° C. After pH adjustment of theresulting suspension to a pH of 2.9 the resulting pH-adjusted suspensionis added to the milling beads (diameter of 0.3 mm) and milling iscarried out in several passages. To the resulting suspension 20 kg ofsodium ascorbate are added. Then water is added and spray drygranulation started. 305 kg of the granules are obtained.

Example 3: Manufacture of Granules of Lutein and Zeaxanthin According tothe Present Invention

160 kg of OSA-Starch, 80 kg of dried glucose syrup and 80 kg of sucroseare dissolved in 480 l of preheated water at 72° C. for at least 30minutes (matrix). 60 kg of FloraGlo lutein crystals (as available fromKemin Foods, Des Moines, US) are then added to the matrix under stirringat a temperature between 39° C. and 21° C. After pH adjustment of theresulting suspension to a pH of 3.03 the resulting pH-adjustedsuspension is added to the milling beads (diameter of 0.3 mm) andmilling is carried out in several passages. To the resulting suspension18 kg of sodium ascorbate are added. Then water is added and spray drygranulation started. 330 kg of the granules are obtained.

Measurement of Particle Size

All particle sizes of the solid particles of the present invention aredetermined by laser diffraction technique using a “Mastersizer 3000” ofMalvern Instruments Ltd., UK. Further information on this particle sizecharacterization method can e.g. be found in “Basic principles ofparticle size analytics”, Dr. Alan Rawle, Malvern Instruments Limited,Enigma Business Part, Grovewood Road, Malvern, Worcestershire, WR14 1XZ,UK and the “Manual of Malvern particle size analyzer”. Particularreference is made to the user manual number MAN 0096, Issue 1.0,November 1994.

Measurement of the Particle Size Distribution

The particle size distribution was measured after the re-dispersedgranules of example 1, 2 and 3, respectively, were treated withultrasound and centrifuged.

Flowability

All three granules manufactured according to examples 1-3 showed anexcellent flowability (see table 1 below).

TABLE 1 Flow [g/min] Example 1 - Example 2 - Example 3 - through anorifice Flow Flow Flow with a diameter of [g/min] [g/min] [g/min] 15 mm2308 2308 2368 10 mm 789 789 796 9 mm 571 657 672 7 mm 300 299 305 5 mm126 126 124

Density

The bulk density and the tapped density of all three examples is high ascan be seen in the following table 2.

TABLE 2 Example 1 Example 2 Example 3 Bulk density 0.71 g/cm³ 0.71 g/cm³0.71 g/cm³ Tapped density 0.79 g/cm³ 0.79 g/cm³ 0.79 g/cm³

Beverages

According to the present invention the “Lutein SG-VG form”(SG=Spray-granulated;

VG=vegetable) with the particle size as given above and as manufacturedaccording to example 1, 2 or 3 can be preferably used to color thefollowing beverages: soft drinks as well as flavored waters, fortifiedwaters, sports drinks, mineral drinks and carbonated beverages. Fruitjuices and fruit-juice containing soft drinks may also be colored.Alcoholic beverages, instant beverage powders, sugar-containingbeverages and diet beverages containing non-calorific or artificialsweeteners represent still further examples of beverages which can becolored by the lutein granules of the present invention.

Soft Drink Application

The soft drink has the following composition:

Ingredient Amount of ingredient 1 Potassium sorbate 0.2 g 2 Sugar syrup(64° Brix) 156.2 g Ascorbic acid 0.2 g Aqueous 50-weight-% 5.0 g citricacid Apricot flavor (water- 0.2 g soluble, Givaudan 10095-36) Stocksolution * 10 g (i.e. 10 ppm) 3 Water Filled up so that a total amountof the soft drink of 1000 ml results Total amount 1000 ml * From thegranules according to example 1, 2 and 3 a stock solution is prepared,whereby the granules are diluted with water so that the stock solutionhas a concentration of the Lutein of 0.1 weight-% (=1000 ppm).

The soft drink is prepared as follows:

Potassium sorbate 1) is dissolved in water, the other ingredients 2) areadded one after the other while the mixture is gently stirred. Then theresulting soft drink syrup is diluted with drink water in such an amountto result in 1000 ml of the soft drink. The pH of the soft drink is inthe range of 2.8 to 3.5.

The soft drink is then filled in a glass bottle and the bottle sealedwith a metallic cap. The bottle is pasteurized for approximately 3minutes at 80° C. using a tunnel pasteurizer (Miele, Switzerland).Colour measurements are performed directly after beverage preparation(time=0).

Color Measurements

Color measurements for the application in food are performed with acolorimeter (Hunter Lab Ultra Scan Pro) which expresses color valuesaccording to the psychophysical perception of color by human eye.

Color measurements are carried out after CIE guidelines (CommissionInternational d'Eclairage). Values can be expressed either as planarcoordinates L*a*b* with L* being the measuring value for lightness, witha*being the value on the red-green-axis and with b* being the value onthe yellow-blue-axis.

Instrument Settings:

Color scale: CIE L*a*b*/L*C*h*

Light source definition: D65 daylight equivalent

Geometry: Diffuse/8°

Wavelengths: scan 350 to 1050 nm in 5 nm optical resolution

Sample measurement area diameter: 19 mm (large)

Calibration mode: Transmission/white tile

The Chroma (C*) sometimes called saturation describes the vividness ordullness of a color which can be calculated as followed:

C*=f(a*2+b*2)

The angle called hue (h) describes how we perceive an object's color andcan be calculated as followed:

h=tan(b/a)(−1)

The color change DE* is calculated as follows:

DE*=√{square root over ((ΔL)²+(Δa)²+(Δb)²)}

Colour Stability:

DE*<3=not visible for the human eye

DE*>3 to 10=visible for the human eye but acceptable

DE*>10=not acceptable

Color values

TABLE 3 Non-pasteurized soft-drink with granules according to example 1Initial After After After value 14 days 30 days 60 days L* 90.19 90.1590.26 90.21 a* 3.75 3.84 3.79 3.80 b* 29.75 30.29 29.95 29.96 C* 29.9930.53 30.19 30.20 h* 82.82 82.77 82.79 82.77 DE* after 60 days = 0.22

TABLE 4 Non-pasteurized soft-drink with granules according to example 2Initial After After After value 14 days 30 days 60 days L* 88.86 88.9388.85 88.99 a* 4.83 4.83 4.87 4.78 b* 36.35 36.30 36.52 36.01 C* 36.6736.62 36.84 36.33 h* 82.43 82.42 82.40 82.44 DE* after 60 days = 0.37

TABLE 5 Non-pasteurized soft-drink with granules according to example 3Initial After After After value 14 days 30 days 60 days L* 89.56 89.5289.53 89.67 a* 4.36 4.39 4.41 4.30 b* 31.62 32.07 31.98 31.59 C* 31.9232.37 32.28 31.88 h* 82.15 82.21 82.15 82.25 DE* after 60 days = 0.13

TABLE 6 Pasteurized soft-drink with granules according to example 1Initial After After After value 14 days 30 days 60 days L* 90.00 90.1790.19 90.26 a* 3.94 3.95 3.81 3.75 b* 30.31 29.63 29.70 29.41 C* 30.5729.89 29.94 29.65 h* 82.59 82.41 82.69 82.73 DE* after 60 days = 0.96

TABLE 7 Pasteurized soft-drink with granules according to example 2Initial After After After value 14 days 30 days 60 days L* 88.72 88.9188.96 88.96 a* 4.96 4.92 4.77 4.75 b* 36.34 35.69 35.50 35.69 C* 36.6836.03 35.82 36.00 h* 82.23 82.15 82.35 82.42 DE* after 60 days = 0.72

TABLE 8 Pasteurized soft-drink with granules according to example 3Initial After After After value 14 days 30 days 60 days L* 89.37 89.4889.63 89.63 a* 4.53 4.52 4.30 4.30 b* 31.82 31.59 31.19 31.25 C* 32.1431.91 31.49 31.54 h* 81.90 81.86 82.15 82.17 DE* after 60 days = 0.67

As can be seen from the values given above, the color is stable over 60days with a DE* in all cases<1.

Turbidity Measurements

Suspended solids (or particles) are responsible for the turbidappearance of beverages containing juice. This turbid appearance can beevaluated by turbidity measurements. Turbidity depends on thelight-scattering properties of such particles: their size, their shapeand their refractive index.

In this work turbidity measurements were conducted using a Turbidimeter(Hach 2100N ISO, USA) and turbidity values were given in NTU(nephelometric turbidity units). Neophelometer measures the lightscattered by a sample in 90° from the incident light path.

Tab. 9 shows the results obtained for the turbidity of thenon-pasteurized soft drinks.

Example 1 Example 2 Example 3 Turbidity initial [NTU] 129.0 134.0 136.0Turbidity after 14 days [NTU] 125.0 131.0 127.0 Turbidity after 30 days[NTU] 121.0 122.0 131.0 Turbidity after 60 days [NTU] 117.0 127.0 119.0

Tab. 10 shows the results obtained for the turbidity of the pasteurizedsoft drinks.

Example 1 Example 2 Example 3 Turbidity initial [NTU] 127.0 131.0 135.0Turbidity after 14 days [NTU] 123.0 130.0 132.0 Turbidity after 30 days[NTU] 122.0 130.0 128.0 Turbidity after 60 days [NTU] 116.0 126.0 127.0

Physical Stability

After 14, 30 and 60 days of storage the non-pasteurized and pasteurizedsoft drinks are evaluated visually concerning their physical appearance.Hereby the samples are examined visually whether they show a ring in thebottle neck, whether they show particles on the surface and whether theyshow white sediments. The following schedule of notes is applied:

Ring in Bottle Neck:

-   6=no ring-   5=hardly noticeable ring-   4=recognizable ring-   3=clear fine ring recognizable-   2=strong ring recognizable-   1=broad ring recognizable

Particles on Surface:

-   6=no particles-   5=1 to 10 particles-   4=more than 10 particles-   3=not countable anymore-   2=half of the surface covered-   1=more than half of the surface covered

Sediment:

-   6=no sediment-   5=slight matt glimmer-   4=fine matt sediment-   3=matt sediment-   2=strong matt sediment-   1=very strong matt sediment

For a good performance, scores should be 3.

Tab. 11 shows the results obtained for the appearance evaluation of thenon-pasteurized soft drinks.

Soft drink containing a Ring in Particles powder according bottle on theWhite to example neck surface sediment 1 (14 days) 4 3 4 1 (30 days) 4 53 1 (60 days) 3 4 4 2 (14 days) 5 4 4 2 (30 days) 5 4 4 2 (60 days) 3 44 3 (14 days) 5 4 4 3 (30 days) 4 4 4 3 (60 days) 3 4 4

The samples show a very good performance with respect to theirappearance attributes.

Tab. 12 shows the results obtained for the appearance evaluation of thepasteurized soft drinks.

Soft drink containing a Ring in Particles powder according bottle on theWhite to example neck surface sediment 1 (14 days) 5 4 4 1 (30 days) 4 44 1 (60 days) 3 3 4 2 (14 days) 5 5 4 2 (30 days) 4 4 5 2 (60 days) 3 54 3 (14 days) 4 3 4 3 (30 days) 4 5 4 3 (60 days) 3 4 4

Also in pasteurized drinks, the samples show a very good performancewith respect to their appearance attributes.

TABLE 13 Chemical stability of the non-pasteurized soft-drinks; given isthe measured amount of lutein in %, based on the initial value InitialAfter After After value 14 days 30 days 60 days Example 1 100.00 95.9392.68 91.06 Example 2 100.00 91.60 90.84 87.79 Example 3 100.00 95.9794.35 88.71

TABLE 14 Chemical stability of pasteurized soft-drinks; given is themeasured amount of lutein in %, based on the initial value Initial AfterAfter After value 14 days 30 days 60 days Example 1 100.00 91.20 92.0089.60 Example 2 100.00 92.25 90.70 84.50 Example 3 100.00 92.86 88.1083.33

Both, pasteurized and non-pasteurized, soft drinks showed a goodchemical stability within 60 days.

1. A beverage comprising a beverage liquid and granules mixed with thebeverage liquid, wherein the granules comprise: (i) a milled carotenoidconsisting of lutein and/or zeaxanthin, wherein the milled carotenoidhas the following particle size distribution: D [3,2] in the range offrom 0.6 to 1.5 μm, and D [v, 0.5] in the range of from 1.1 to 3.5 μm,(ii) a matrix material which encapsulates the milled carotenoid andcomprises at least one modified food starch, a glucose syrup andsucrose, and (iii) a water-soluble antioxidant, wherein the granuleshave the following particle size distribution: D [3,2] in the range offrom 200 to 300 μm, and D [v, 0.5] in the range of from 220 to 320 μm,and wherein all D values are as measured by laser diffraction accordingto the Fraunhofer scattering model, and wherein the granules do notinclude an oil or a gelatin.
 2. The beverage according to claim 1,wherein the beverage is a soft drink having a pH in the range of from 2to
 5. 3. The beverage according to claim 1, wherein the beverage has acolor stability DE* 1 for 60 days.
 4. The beverage according to claim 1,wherein the beverage has a turbidity 150 NTU.
 5. The beverage accordingto claim 1, wherein the amount of the milled carotenoid, the amount ofthe modified food starch, the amount of the glucose syrup, the amount ofsucrose and the amount of the water-soluble antioxidant are together atleast 90 wt. % of the total weight of the granules.
 6. The beverageaccording to claim 1, wherein the amount of the milled carotenoid, theamount of the modified food starch, the amount of the glucose syrup, theamount of sucrose and the amount of the water-soluble antioxidant aretogether at least 95 wt. % of the total weight of the granules.
 7. Thebeverage according to claim 1, wherein the amount of modified foodstarch in kilograms is the same as the total amount of glucose syrup andsucrose in kilograms.
 8. The beverage according to claim 1, wherein thegranules have the following particle size distribution: D [3,2] in therange of from 230 to 270 μm, and D [v, 0.5] in the range of from 240 to290 μm.
 9. The beverage according to claim 1, wherein the milledcarotenoid has the following particle size distribution: D [3,2] in therange of from 0.8 to 1.2 μm, and D [v, 0.5] in the range of from 1.1 to2.6 μm.
 10. The beverage according to claim 1, wherein the amount of themilled carotenoid in the granules is in a range of from 1-30 wt. %,based on the total weight of the granules.
 11. The beverage according toclaim 1, wherein the amount of the modified food starch is in a therange of from 10 to 50 weight-%, based on the total weight of thegranules.
 12. The beverage according to claim 1, wherein the amount ofthe glucose syrup is in a range of from 5 to 40 wt. %, based on thetotal weight of the granules.
 13. The beverage according to claim 1,wherein the amount of sucrose is in a range of from 5 to 40 wt. %, basedon the total weight of the granules.
 14. The beverage according to claim1, wherein the amount of the water-soluble anti-oxidant is in a range offrom 0.1 to 10 wt. %, based on the total weight of the granules.
 15. Thebeverage according to claim 1, wherein the granules have a flowabilityof at least 100 g/min through an orifice with a diameter of 5 mm. 16.The beverage according to claim 1, wherein the granules do not compriseany of the following compounds: hydrolyzed lecithin products, GumArabic, fat-soluble antioxidants, isomalt, μ-zeacarotene andμ-zeacarotene.
 17. The beverage according to claim 1, wherein theglucose syrup has a dextrose equivalent (DE) in a range of from 20 to95.
 18. The beverage according to claim 1, wherein the glucose syrup iscomprised of a mixture of a low dextrose equivalent (DE) glucose syruphaving a DE in a range of from 20 to 25, and a high DE glucose syruphaving a DE in a range of from 90 to
 100. 19. A process for themanufacture of granules which are comprised of: (i) a milled carotenoidconsisting of lutein and/or zeaxanthin, wherein the milled carotenoidhas the following particle size distribution: D [3,2] in the range offrom 0.6 to 1.5 μm, and D [v, 0.5] in the range of from 1.1 to 3.5 μm,(ii) a matrix material which encapsulates the milled carotenoid andcomprises at least one modified food starch, a glucose syrup andsucrose, and (iii) a water-soluble antioxidant, wherein the granuleshave the following particle size distribution: D [3,2] in the range offrom 200 to 300 μm, and D [v, 0.5] in the range of from 220 to 320 μm,and wherein all D values are as measured by laser diffraction accordingto the Fraunhofer scattering model, and wherein the granules do notinclude an oil or a gelatin, wherein the process comprises the steps of:a) providing an aqueous solution of at least one modified food starch, aglucose syrup and sucrose; b) adding the carotenoid selected from thegroup consisting of lutein and zeaxanthin and any mixture thereof to thesolution of step a) hereby obtaining a suspension; c) milling thesuspension of step b) until the following particle size distribution ofthe milled carotenoid is reached: D [3,2] in the range of from 0.6 to1.5 μm, and D [v, 0.5] in the range of from 1.1 to 3.5 μm, wherein bothD values are as measured by laser diffraction (Malvern Instruments Ltd,Malvern, UK, Mastersizer 3000) according to the Fraunhofer scatteringmodel; and d) spray-granulating the suspension of step c) to obtain thegranules; and wherein the process further comprises adding awater-soluble antioxidant.